RESUMEN
The residual stress generated during heat treatment of nickel-base superalloys will affect their service performance and introduce primary cracks. In a component with high residual stress, a tiny amount of plastic deformation at room temperature can release the stress to a certain extent. However, the stress-releasing mechanism is still unclear. In the present study, the micro-mechanical behavior of the FGH96 nickel-base superalloy during room temperature compression was studied using in situ synchrotron radiation high-energy X-ray diffraction. The in situ evolution of the lattice strain was observed during deformation. The stress distribution mechanism of grains and phases with different orientations was clarified. The results show that at the elastic deformation stage, the (200) lattice plane of γ' phase bears more stress after the stress reaches 900 MPa. When the stress exceeds 1160 MPa, the load is redistributed to the grains with their <200> crystal directions aligned with the loading direction. After yielding, the γ' phase still bears the main stress.
RESUMEN
Structure-sensitive catalyzed reactions can be influenced by a number of parameters. So far, it has been established that the formation of Pd-C species is responsible for the behavior of Pd nanoparticles employed as catalysts in a butadiene partial hydrogenation reaction. In this study, we introduce some experimental evidence indicating that subsurface Pd hydride species are governing the reactivity of this reaction. In particular, we detect that the extent of formation/decomposition of PdHx species is very sensitive to the Pd nanoparticle aggregate dimensions, and this finally controls the selectivity in this process. The main and direct methodology applied to determine this reaction mechanism step is time-resolved high-energy X-ray diffraction (HEXRD).
RESUMEN
Amorphous bulk metallic glasses with the composition Fe48Cr15Mo14C15B6Y2have been of interest due to their special mechanical and electronic properties, including corrosion resistance, high yield-strength, large elasticity, catalytic performance, and soft ferromagnetism. Here, we apply a reverse Monte Carlo technique to unravel the atomic structure of these glasses. The pair-distribution functions for various atomic pairs are computed based on the high-energy x-ray diffraction data we have taken from an amorphous sample. Monte Carlo cycles are used to move the atomic positions until the model reproduces the experimental pair-distribution function. The resulting fitted model is consistent with ourab initiosimulations of the metallic glass. Our study contributes to the understanding of functional properties of Fe-based bulk metallic glasses driven by disorder effects.
RESUMEN
Cathode catalyst layers of proton exchange membrane fuel cells (PEMFCs) typically consist of carbon-supported platinum catalysts with varying weight ratios of proton-conducting ionomers. N-Doping of carbon support materials is proposed to enhance the performance and durability of the cathode layer under operating conditions in a PEMFC. However, a detailed understanding of the contributing N-moieties is missing. Here, we report the successful synthesis and fuel cell implementation of Pt electrocatalysts supported on N-doped carbons, with a focus on the analysis of the N-induced effect on catalyst performance and durability. A customized fluidized bed reduction reactor was used to synthesize highly monodisperse Pt nanoparticles deposited on N-doped carbons (N-C), the catalytic oxygen reduction reaction activity and stability of which matched those of state-of-the-art PEMFC catalysts. Operando high-energy X-ray diffraction experiments were conducted using a fourth generation storage ring; the light of extreme brilliance and coherence allows investigating the impact of N-doping on the degradation behavior of the Pt/N-C catalysts. Tests in liquid electrolytes were compared with tests in membrane electrode assemblies in single-cell PEMFCs. Our analysis refines earlier views on the subject of N-doped carbon catalyst supports: it provides evidence that heteroatom doping and thus the incorporation of defects into the carbon backbone do not mitigate the carbon corrosion during high-potential cycling (1-1.5 V) and, however, can promote the cell performance under usual PEMFC operating conditions (0.6-0.9 V).
RESUMEN
Al-Cu-Li alloys are famous for their high strength, ductility and weight-saving properties, and have for many years been the aerospace alloy of choice. Depending on the alloy composition, this multi-phase system may give rise to several phases, including the major strengthening T1 (Al2CuLi) phase. Microstructure investigations have extensively been reported for conventionally processed alloys with little focus on their Additive Manufacturing (AM) characterised microstructures. In this work, the Laser Powder Bed Fusion (LPBF) built microstructures of an AA2099 Al-Cu-Li alloy are characterised in the as-built (no preheating) and preheat-treated (320 °C, 500 °C) conditions using various analytical techniques, including Synchrotron High-Energy X-ray Diffraction (S-HEXRD). The observed dislocations in the AM as-built condition with no detected T1 precipitates confirm the conventional view of the difficulty of T1 to nucleate on dislocations without appropriate heat treatments. Two main phases, T1 (Al2CuLi) and TB (Al7.5Cu4Li), were detected using S-HEXRD at both preheat-treated temperatures. Higher volume fraction of T1 measured in the 500 °C (75.2 HV0.1) sample resulted in a higher microhardness compared to the 320 °C (58.7 HV0.1) sample. Higher TB volume fraction measured in the 320 °C sample had a minimal strength effect.
RESUMEN
Atomic layer deposition (ALD) is a well-established technique for depositing nanoscale coatings with pristine control of film thickness and composition. The trimethylaluminum (TMA) and water (H2O) ALD chemistry is inarguably the most widely used and yet to date, we have little information about the atomic-scale structure of the amorphous aluminum oxide (AlOx) formed by this chemistry. This lack of understanding hinders our ability to establish process-structure-property relationships and ultimately limits technological advancements employing AlOx made via ALD. In this work, we employ synchrotron high-energy X-ray diffraction (HE-XRD) coupled with pair distribution function (PDF) analysis to characterize the atomic structure of amorphous AlOx ALD coatings. We combine ex situ and in operando HE-XRD measurements on ALD AlOx and fit these experimental data using stochastic structural modeling to reveal variations in the Al-O bond length, Al and O coordination environment, and extent of Al vacancies as a function of growth conditions. In particular, the local atomic structure of ALD AlOx is found to change with the substrate and number of ALD cycles. The observed trends are consistent with the formation of bulk Al2O3 surrounded by an O-rich surface layer. We deconvolute these data to reveal atomic-scale structural information for both the bulk and surface phases. Overall, this work demonstrates the usefulness of HE-XRD and PDF analysis in improving our understanding of the structure of amorphous ALD thin films and provides a pathway to evaluate how process changes impact the structure and properties of ALD films.
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The aim of this work is to investigate quench induced precipitation during continuous cooling in aluminium wrought alloys EN AW-7150 and EN AW-6082 using in situ synchrotron wide-angle X-ray scattering (WAXS). While X-ray diffraction is usually an ex situ method, a variety of diffraction patterns were recorded during the cooling process, allowing in situ analysis of the precipitation process. The high beam energy of about 100 keV allows the beam to penetrate a bulk sample with a 4 mm diameter in a quenching dilatometer. Additionally, the high intensity of a synchrotron source enables sufficiently high time resolution for fast in situ cooling experiments. Reaction peaks could be detected and compared with results from differential scanning calorimetry (DSC) by this method. A methodology is presented in this paper to evaluate WAXS data in a way that is directly comparable to DSC-experiments. The results show a high correlation between both techniques, DSC and WAXS, and can significantly improve continuous cooling precipitation diagrams.
RESUMEN
Quenching and Partitioning (Q&P) steels are promising candidates for automotive applications because of their lightweight potential. Their properties depend on carbon enrichment in austenite which, in turn, is strongly influenced by carbide precipitation in martensite during quenching and partitioning treatment. In this paper, by coupling in situ High Energy X-Ray Diffraction (HEXRD) experiments and Transmission Electron Microscopy (TEM), we give some clarification regarding the precipitation process of iron carbides in martensite throughout the Q&P process. For the first time, precipitation kinetics was followed in real time. It was shown that precipitation starts during the reheating sequence for the steel studied. Surprisingly, the precipitated fraction remains stable all along the partitioning step at 400 °C. Furthermore, the analyses enable the conclusion that the iron carbides are most probably eta carbides. The presence of cementite was ruled out, while the presence of several epsilon carbides cannot be strictly excluded.